CN113117442A - Tail gas treatment method and system in polycrystalline silicon production - Google Patents
Tail gas treatment method and system in polycrystalline silicon production Download PDFInfo
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Abstract
The invention provides a tail gas treatment method and a tail gas treatment system in polycrystalline silicon production, wherein the method comprises the following steps: introducing the mixed gas to be treated into a first separation device to obtain first treated mixed gas and silicon powder solid slag; discharging the silicon powder solid slag to a residue treatment device; introducing the first treated mixed gas into a quenching tower to obtain first chlorosilane gas and chlorosilane residual liquid containing impurities; collecting the first chlorosilane gas, condensing the first chlorosilane gas into first liquid-phase chlorosilane, and conveying the first liquid-phase chlorosilane to the first separation device; introducing the chlorosilane residual liquid into a second separation device, and carrying out solid-liquid separation on the chlorosilane residual liquid in the second separation device to obtain a chlorosilane clear liquid and a silicon powder turbid liquid; conveying the chlorosilane clear liquid to a quenching tower; and discharging the silicon powder turbid liquid to a residue treatment device. The embodiment of the disclosure can at least solve the problems of shortened operation period of pipelines and equipment, overhigh maintenance cost and the like caused by overhigh solid content of chlorosilane in the related technology.
Description
Technical Field
The disclosure relates to the technical field of polycrystalline silicon production, in particular to a tail gas treatment method in polycrystalline silicon production and a tail gas treatment system in polycrystalline silicon production.
Background
With the gradual exhaustion of fossil energy and the increasing aggravation of environmental pollution problems, it is urgent to search for a pollution-free renewable energy source. Solar energy is taken as the most abundant renewable energy, compared with other energy sources, the solar energy has the advantages of cleanliness, safety, universality, resource sufficiency, potential economy and the like, the solar energy is fully utilized, and the solar energy has important economic and strategic significance for realizing sustainable development in a low-carbon mode.
The main raw materials of the solar photovoltaic cell produced by polysilicon have the production cost of trichlorosilane synthesis process nearly consistent with that of each manufacturer along with the continuous optimization of the polysilicon production process, and the production cost of the overhaul cost for tail gas treatment in polysilicon production gradually becomes the biggest obstacle for limiting the further reduction of the polysilicon production cost. Although various manufacturers continuously research and search the synthesis process, it is very effective to reduce the solid content of the tail gas treatment equipment and the pipeline inlet, and in the tail gas treatment process in the production of polycrystalline silicon, the equipment is worn due to the high solid content of the equipment and the pipeline inlet, the service life of the pipeline and the equipment is shortened, and even potential safety hazards are caused.
Therefore, how to prolong the service life of pipelines and equipment for tail gas treatment in the production of polycrystalline silicon so as to reduce the production cost of polycrystalline silicon is a problem to be solved urgently at present.
Disclosure of Invention
The present disclosure provides a tail gas treatment method and system in polysilicon production, which can prolong the service life of pipelines and equipment, thereby reducing the production cost of polysilicon.
According to an aspect of the embodiments of the present disclosure, there is provided a method for treating tail gas in polysilicon production, including:
introducing the mixed gas to be treated into a first separation device, and carrying out primary spraying and washing on the mixed gas to be treated in the first separation device to obtain first treated mixed gas and silicon powder solid slag;
discharging the silicon powder solid slag to a residue treatment device; and the number of the first and second groups,
introducing the first treated mixed gas into a quenching tower, and spraying and washing the first treated mixed gas in the quenching tower to obtain a first chlorosilane gas and a chlorosilane residual liquid containing impurities;
collecting the first chlorosilane gas, condensing the first chlorosilane gas into first liquid-phase chlorosilane, and conveying the first liquid-phase chlorosilane to the first separation device; and the number of the first and second groups,
introducing the chlorosilane residual liquid into a second separation device, and carrying out solid-liquid separation on the chlorosilane residual liquid in the second separation device to obtain a chlorosilane clear liquid and a silicon powder turbid liquid;
conveying the chlorosilane clear liquid to a quenching tower; and the number of the first and second groups,
and discharging the silicon powder turbid liquid to a residue treatment device.
In one embodiment, the preliminary spraying and washing of the mixed gas to be treated in the first separation device is performed to obtain a first treated mixed gas and solid slag of silicon powder, specifically:
carrying out primary spraying and washing on the treated mixed gas in the first separation device to obtain a second treated mixed gas and silicon powder solid slag; and the number of the first and second groups,
and carrying out secondary spraying and washing on the second treated mixed gas in the first separation device to obtain the first treated mixed gas and silicon powder solid slag.
In one embodiment, before discharging the solid silicon powder slag to a residue treatment device, the method further comprises:
discharging the silicon powder solid slag to a transfer tank, and flashing the silicon powder solid slag in the transfer tank to obtain second chlorosilane gas; and the number of the first and second groups,
introducing the second chlorosilane gas into a filter, and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen in the filter to obtain filtered second chlorosilane gas and hydrogen mixed gas;
introducing the filtered second chlorosilane gas and hydrogen mixed gas into a second cooler, and cooling the second chlorosilane gas and hydrogen mixed gas in the second cooler to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
introducing the second liquid-phase chlorosilane into a liquid seal device for recycling; and the number of the first and second groups,
and introducing the gas-phase hydrogen into a hydrogen make-up foretank for recycling.
In one embodiment, before discharging the turbid liquid of silicon powder to a residue treatment device, the method further comprises:
discharging the silicon powder turbid liquid to a transfer tank, and flashing the silicon powder turbid liquid in the transfer tank to obtain second chlorosilane gas; and the number of the first and second groups,
introducing the second chlorosilane gas into a filter, and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen in the filter to obtain filtered second chlorosilane gas and hydrogen mixed gas;
introducing the filtered second chlorosilane gas and hydrogen mixed gas into a second cooler, and cooling the second chlorosilane gas and hydrogen mixed gas in the second cooler to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
introducing the second liquid-phase chlorosilane into a liquid seal device for recycling; and the number of the first and second groups,
and introducing the gas-phase hydrogen into a hydrogen make-up foretank for recycling.
According to another aspect of the embodiments of the present disclosure, there is provided a system for treating tail gas in polysilicon production, including:
the first separation device is used for obtaining mixed gas to be treated and carrying out primary spraying and washing on the mixed gas to be treated to obtain first treated mixed gas and silicon powder solid slag;
the quenching tower is connected with the first separation device and used for obtaining the first treated mixed gas and spraying and washing the first treated mixed gas to obtain a first chlorosilane gas and a chlorosilane residual liquid containing impurities;
the collecting device is connected with the quenching tower and is used for collecting the first chlorosilane gas, condensing the first chlorosilane gas into first liquid-phase chlorosilane and conveying the first liquid-phase chlorosilane to the first separating device;
the second separation device is respectively connected with the quenching tower and the residue treatment device, is used for carrying out solid-liquid separation on the chlorosilane residual liquid to obtain a chlorosilane clear liquid and a silicon powder turbid liquid, and is also used for conveying the chlorosilane clear liquid to the quenching tower; and the number of the first and second groups,
and the residue treatment device is respectively connected with the first separation device and the second separation device and is used for collecting and treating the silicon powder solid residues from the first separation device and the silicon powder turbid liquid from the second separation device.
In one embodiment, the second separation device is a cyclone.
In one embodiment, the first separation device comprises a venturi quench tank and a venturi separation tank;
the Venturi quenching tank is respectively connected with the Venturi separation tank and the residue treatment device and is used for obtaining mixed gas to be treated and carrying out primary spraying and washing on the treated mixed gas to obtain second treated mixed gas and silicon powder solid residues; and the number of the first and second groups,
the Venturi quenching tank is also used for conveying the second processing mixed gas to the Venturi separation tank and discharging the silicon powder solid slag to the slag processing device;
the venturi separation tank is respectively connected with the venturi quenching tank and the quenching tower and is used for obtaining the second processing mixed gas and carrying out secondary spraying and washing on the second processing mixed gas to obtain the first processing mixed gas and silicon powder solid slag; and the number of the first and second groups,
the Venturi separation tank is also used for conveying the first treated mixed gas to the quenching tower and discharging the silicon powder solid slag to the slag treatment device.
In one embodiment, the system further comprises: and the quenching tower circulating pump is respectively connected with the quenching tower and the second separation device and is used for pressurizing and conveying the chlorosilane clear liquid output by the second separation device to the quenching tower.
In one embodiment, the quench tower circulation pump employs an open impeller; and/or the circulating pump motor of the quenching tower adopts a frequency conversion mode; and/or the circulating pump of the quenching tower is made of alloy materials.
In one embodiment, the collection device comprises:
a first cooler for cooling the first chlorosilane gas to obtain a first liquid phase chlorosilane; and the number of the first and second groups,
and the condensate intermediate tank is used for collecting the first liquid-phase chlorosilane and conveying the first liquid-phase chlorosilane to the first separation device.
In one embodiment, the system further comprises:
the transfer tank is connected between the first separation device and the residue treatment device and is used for flashing the silicon powder solid residue into second chlorosilane gas;
the filter is connected with the transfer tank and is used for introducing the second chlorosilane gas and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen to obtain filtered second chlorosilane gas and hydrogen mixed gas;
the second cooler is connected with the filter and used for cooling the second chlorosilane gas and hydrogen mixed gas to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
the liquid seal device is respectively connected with the second cooler and the transfer tank and is used for recovering the second liquid-phase chlorosilane and returning the second liquid-phase chlorosilane to the transfer tank; and the number of the first and second groups,
a make-up hydrogen front tank connected to the second cooler for recovering the gas-phase hydrogen gas.
In one embodiment, the system further comprises:
the transfer tank is connected between the second separation device and the residue treatment device and is used for flashing the turbid liquid of the silicon powder out of a second chlorosilane gas;
the filter is connected with the transfer tank and is used for introducing the second chlorosilane gas and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen to obtain filtered second chlorosilane gas and hydrogen mixed gas;
the second cooler is connected with the filter and used for cooling the second chlorosilane gas and hydrogen mixed gas to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
the liquid seal device is respectively connected with the second cooler and the transfer tank and is used for recovering the second liquid-phase chlorosilane and returning the second liquid-phase chlorosilane to the transfer tank; and the number of the first and second groups,
a make-up hydrogen front tank connected to the second cooler for recovering the gas-phase hydrogen gas.
In one embodiment, the system further comprises: and the silicon powder storage tank is respectively connected with the second separation device and the transfer tank and is used for depositing the silicon powder turbid liquid and introducing the deposited silicon powder turbid liquid into the transfer tank.
The technical scheme provided by the embodiment of the disclosure can have the following beneficial effects:
the tail gas treatment method in polysilicon production provided by the embodiment of the disclosure comprises the steps of introducing a gas mixture to be treated into a first separation device, primarily spraying and washing the gas mixture to be treated in the first separation device, introducing the primarily sprayed and washed gas mixture into a quenching tower, washing solid impurities containing a large amount of silicon powder and other metal chlorides, reducing the solid content of the gas mixture, after the gas mixture enters the quenching tower for quenching, carrying out solid-liquid separation on chlorosilane residual liquid at the bottom of the quenching tower by using a second separation device, separating the residual solid impurities from chlorosilane liquid, conveying the separated chlorosilane clear liquid to the quenching tower, depositing the silicon powder, metal chlorides and other solid impurities in the chlorosilane residual liquid in the process into the silicon powder solid residue and the silicon powder turbid liquid, greatly reducing the solid content of chlorosilane, and solving the abnormal operation of the quenching tower caused by the excessively high solid content in the related technology, and the running period of pipelines and equipment such as a circulating pump of the quenching tower is shortened, so that the production cost of the polycrystalline silicon is reduced.
Additional features and advantages of the disclosure will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the disclosure. The objectives and other advantages of the disclosure may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
The accompanying drawings are included to provide a further understanding of the disclosed embodiments and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the example serve to explain the principles of the disclosure and not to limit the disclosure.
Fig. 1 is a schematic flow chart of a method for treating tail gas in polysilicon production according to an embodiment of the present disclosure;
fig. 2 is a schematic structural diagram of a tail gas treatment system in polysilicon production according to an embodiment of the present disclosure.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, specific embodiments of the present disclosure are described below in detail with reference to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present disclosure, are given by way of illustration and explanation only, not limitation.
It should be noted that, in the present disclosure, the embodiments and features of the embodiments may be arbitrarily combined with each other without conflict.
In which the terminology used in the embodiments of the disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used in the disclosed embodiments and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The tail gas generated by synthesis in the cold hydrogenation production of polysilicon (hereinafter referred to as the mixed gas to be treated) mainly comprises: silicon powder, metal chloride, polymer, high-boiling-point substance and chlorosilane compound. The metal chloride is aluminum chloride and/or calcium chloride; the polymer is a polymer of phosphorus trichloride and/or a polymer of boron trichloride; the high-boiling-point substance is aluminum chloride, ferric chloride and/or calcium chloride; the chlorosilane compound is trichlorosilane and/or silicon tetrachloride. The silicon powder, the metal chloride, the polymer and the high-boiling-point substance are easy to be changed into sticky substances after being cooled due to high boiling points, so that pipelines are blocked, and the normal operation of production is seriously influenced. Because the polycrystalline silicon cold hydrogenation production yield is high, the working pressure is high, the content of the impurities in the tail gas generated by synthesis in the cold hydrogenation production is high, the conditions of short running time of pipelines and equipment such as a circulating pump of a production quenching tower and the like, high production unit consumption and the like can be caused according to the tail gas treatment mode in the related technology, and safety accidents are easy to occur.
To solve the above problem, referring to fig. 1, fig. 1 is a schematic flow chart of a method for treating tail gas in polysilicon production according to an embodiment of the present disclosure, as shown in fig. 1, the method includes steps S101 to S108.
It should be noted that, the reference numbers and the sequence of the steps in the present embodiment are only for convenience of description of the present embodiment, and do not specifically limit the steps, and in some examples, the following steps may be in other sequences.
In step S101, the mixed gas to be treated is introduced into a first separation device, and the mixed gas to be treated is subjected to preliminary spray washing in the first separation device, so as to obtain a first treated mixed gas and solid silicon powder slag.
In this embodiment, at first let in first separator with the mist to be handled and carry out gas-solid separation, compare in the correlation technique, directly let in the mist to be handled and carry out quench cooling, washing in quench tower, a large amount of silica flour solid residues in the mist has subsided in first separator effectively reduce the solid content of letting in the mist of quench tower, alleviate quench tower circulating pump operating pressure.
Specifically, the first separation device in this embodiment may be a dust removal device for removing solid impurities in the gas mixture to be treated based on the venturi effect, and in this embodiment, the solid impurities in the gas mixture to be treated are removed by spraying chlorosilane liquid in the first separation device, specifically, water spraying is a solution absorption method, and the first separation device has a strong adaptability to dust concentration, and not only can remove coarse solid impurities, but also can remove soluble components in the exhaust gas sufficiently to achieve an effect of purifying air, and in addition, can remove other harmful gases by circulating liquid.
In this embodiment, the preliminary spraying and washing of the gas mixture to be treated in the first separation device to obtain a first treated gas mixture and solid slag of silicon powder specifically includes:
and carrying out primary spraying and washing on the mixed gas to be treated by using chlorosilane liquid in the first separation device to obtain first treated mixed gas and silicon powder solid slag.
In this embodiment, in order to further reduce the solid content in the gas mixture, first separator includes venturi quench jar and venturi knockout drum, let in the gas mixture of treating into first separator, and to in the first separator carry out preliminary spray washing to the gas mixture of treating, obtain first processing gas mixture and silica flour solid sediment, specifically be following step:
introducing the mixed gas to be treated into a Venturi quenching tank, and carrying out primary spraying and washing on the treated mixed gas in the Venturi quenching tank to obtain a second treated mixed gas and silicon powder solid slag;
and introducing the second treated mixed gas into a Venturi separation tank, and carrying out secondary spraying and washing on the second treated mixed gas in the Venturi separation tank to obtain the first treated mixed gas and the silicon powder solid slag.
Specifically, the mixed gas to be treated is firstly introduced into a venturi quenching tank, the venturi quenching tank adopts a post-cooling system chlorosilane for spraying and quenching, silicon powder and metal impurities in the mixed gas to be treated are settled, and a second treated mixed gas and silicon powder solid slag are obtained.
It can be understood that in the process of treating the mixed gas by the venturi quenching tank and the venturi separating tank, the turbid liquid of the solid silicon powder residues is obtained firstly, and because the temperatures in the venturi quenching tank and the venturi separating tank are higher, the moisture in the turbid liquid of the solid silicon powder residues can be vaporized along with the temperatures, and the solid silicon powder residues containing a small amount of liquid can be obtained by sedimentation in the venturi quenching tank and the venturi separating tank.
In step S102, the silicon powder solid slag is discharged to a residue treatment device.
Wherein, the residue treatment device is a slurry stirring tank.
In some embodiments, the venturi quench tank and the venturi separation tank are provided with a discharge valve at the bottom, and the discharge valve is opened to discharge the residue to the residue treatment device by using the pressure difference between the venturi quench tank and the venturi separation tank and the residue treatment device.
In this embodiment, the solid silicon powder residues separated by the first separation device, due to the spraying effect of the chlorosilane liquid, remain chlorosilane compounds in the solid silicon powder residues, and in order to achieve recycling of chlorosilane, in this embodiment, before the solid silicon powder residues are discharged to the residue treatment device, the solid silicon powder residues are firstly introduced into the transfer tank to treat and recycle the solid silicon powder residues, specifically, before the solid silicon powder residues are discharged to the residue treatment device, the method further includes the following steps:
a. and discharging the silicon powder solid slag to a transfer tank, and flashing the silicon powder solid slag in the transfer tank to obtain second chlorosilane gas.
In this embodiment, the solid slag of silicon powder is firstly introduced into the transfer pot, and the chlorosilane liquid remaining in the solid slag of silicon powder is flashed to generate the second chlorosilane gas, and it can be understood that the principle of the flash evaporation is that after the high-pressure saturated liquid enters the relatively low-pressure container, the saturated liquid is changed into a part of saturated vapor and saturated liquid under the pressure of the container due to the sudden pressure reduction.
b. And introducing the second chlorosilane gas into a filter, and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen in the filter to obtain a filtered second chlorosilane gas and hydrogen mixed gas.
In practical application, the second chlorosilane gas that obtains through the flash distillation carries partial dust usually secretly, and this embodiment is through letting in second chlorosilane gas the filter in the processing of removing dust, and this embodiment sets up high-pressure hydrogen in the filter and removes dust to second chlorosilane gas, specifically, adopts high-pressure hydrogen blowback dust, makes the dust blow away second chlorosilane gas, obtains comparatively pure chlorosilane gas and hydrogen gas mixture.
c. And introducing the filtered second chlorosilane gas and hydrogen mixed gas into a second cooler, and cooling the second chlorosilane gas and hydrogen mixed gas in the second cooler to obtain second liquid-phase chlorosilane and gas-phase hydrogen.
In this embodiment, the second cooler condenses the filtered second chlorosilane gas and the hydrogen gas mixture by using chilled water at-20 ℃, and the second chlorosilane gas is converted into second liquid-phase chlorosilane by condensation, which can be understood that the state of hydrogen gas does not change at this temperature.
d. And introducing the second liquid-phase chlorosilane into a liquid seal device for recycling.
Specifically, the second liquid-phase chlorosilane obtained after treatment flows into a transfer tank through a sealing device so as to facilitate the production system to recycle chlorosilane liquid.
e. And introducing the gas-phase hydrogen into a hydrogen make-up foretank for recycling.
The hydrogen is an important raw material in cold hydrogenation production, and the treated gas-phase hydrogen is introduced into the hydrogen make-up front tank and returned to the production system for recycling.
In step S103, the first treated mixed gas is introduced into a quench tower, and the first treated mixed gas is sprayed and washed in the quench tower, so as to obtain a first chlorosilane gas and a chlorosilane residual liquid containing impurities.
Compared with the prior art, the mixed gas to be treated is directly introduced into the quenching tower for treatment, and the treated mixed gas is introduced into the quenching tower in the embodiment, so that the solid content of the mixed gas is greatly reduced, and the operating pressure of the quenching tower and the chlorosilane conveying equipment is relieved.
In step S104, the first chlorosilane gas is collected, condensed into first liquid-phase chlorosilane, and then transported to the first separation device.
In some embodiments, step S104 includes the steps of:
introducing the first chlorosilane gas into a first cooler to obtain first liquid-phase chlorosilane;
and introducing the first liquid-phase chlorosilane into a condensate intermediate tank, and conveying the first liquid-phase chlorosilane to the first separation device through a condensate intermediate tank reflux pump so that the first liquid-phase chlorosilane performs primary spray washing on the mixed gas to be treated in the first separation device.
The first cooler is an air condenser, chlorosilane gas obtained after treatment of the quenching tower is recyclable gas, chlorosilane liquid is required to be used for washing in the first separation device, the first cooler and the condensate intermediate tank are arranged between the quenching tower and the first separation device, the first cooler is used for condensing gas-phase chlorosilane to obtain first liquid-phase chlorosilane, the condensate intermediate tank reflux pump is used for circulating the first liquid-phase chlorosilane, mixed gas in the first separation device is sprayed and washed, tail gas treatment efficiency in polycrystalline silicon production is improved, and resource utilization rate is improved.
In step S105, the chlorosilane residual liquid is introduced into a second separation device, and the chlorosilane residual liquid is subjected to solid-liquid separation in the second separation device to obtain a chlorosilane clear liquid and a silicon powder turbid liquid.
It can be understood, contain silica flour in the chlorosilane raffinate after first processing gas mixture sprays the washing through the quench tower, metal chloride and chlorosilane compound, because it can't be through filtering complete filtering, lead to solid content in the filtrating higher, continuous going on along with production and tail gas treatment, a large amount of silica flour and metal chloride impurity are accumulated, deposit to the quench tower cauldron, pipeline and equipment are extremely easily blockked up to slight dust and metal chloride, be difficult to realize continuous production, it is big to overhaul the degree of difficulty, the maintenance cost is high, not only influence quench tower even running, the extension of restriction quench tower circulating pump duty cycle simultaneously. In order to solve the above problems, in this embodiment, the chlorosilane residual liquid at the bottom of the quenching tower kettle is introduced into the second separation device, the chlorosilane residual liquid is subjected to solid-liquid separation by using the second separation device, solid impurities containing a large amount of silicon powder and other metal chlorides are separated from the chlorosilane clear liquid, the separated chlorosilane clear liquid is conveyed to the inlet of the circulating pump of the quenching tower and is circulated to the quenching tower by the circulating pump, and the silicon powder, the metal chlorides and other solid impurities in the chlorosilane residual liquid are deposited in the turbid liquid of the silicon powder, so that the solid content of the chlorosilane is further reduced, the problems that the operation of the quenching tower is abnormal due to the overhigh solid content of the chlorosilane in the related art, the operation period of the circulating pump of the quenching tower is shortened, and the maintenance cost is reduced.
In step S106, the chlorosilane clear solution is conveyed to a quench tower.
Specifically, the upper chlorosilane clear liquid separated by the second separation device enters a circulating pump of a quenching tower, is circulated and enters the quenching tower, and continues to spray and wash the mixed gas entering the quenching tower, so that the solid content of the upper chlorosilane clear liquid is less, and the circulating pump of the quenching tower cannot cause impeller abrasion or volute abrasion due to conveying solid slag.
In step S107, the silicon powder turbid liquid is discharged to a residue treatment apparatus.
In one embodiment, to further recycle chlorosilane, the method further comprises the following steps before discharging the turbid liquid of silicon powder to a residue treatment device:
discharging the silicon powder turbid liquid to a silicon powder storage tank to deposit silicon powder impurities in the silicon powder storage tank;
in some embodiments, still be provided with middle holding vessel between second separator and silicon powder holding vessel, utilize middle holding vessel to collect probably not separating complete chlorosilane clear liquid in the turbid liquid of silicon powder to through the pressure differential between middle holding vessel and the silicon powder holding vessel, let in the turbid liquid of silicon powder after will collecting and cushion in the silicon powder holding vessel, reuse the pressure differential between silicon powder holding vessel and the middle transfer tank and get into in the transfer tank, through the chlorosilane clear liquid in further collecting the turbid liquid of silicon powder, with the solid content that promotes the turbid liquid of silicon powder, can directly discharge to the transfer tank through the pressure drop, improve the turbid liquid treatment effeciency of silicon powder.
Introducing the deposited turbid liquid of the silicon powder into a transfer tank, and flashing to obtain a second chlorosilane gas in the transfer tank;
introducing the second chlorosilane gas into a filter, and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen in the filter to obtain filtered second chlorosilane gas and hydrogen mixed gas;
introducing the filtered second chlorosilane gas and hydrogen mixed gas into a second cooler, and cooling the second chlorosilane gas and hydrogen mixed gas by using the second cooler to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
introducing the second liquid-phase chlorosilane into a liquid seal device for recycling; and the number of the first and second groups,
and introducing the gas-phase hydrogen into a hydrogen make-up foretank for recycling.
It should be noted that the method for processing the turbid liquid of silicon powder in the process is substantially the same as the method for processing the solid residue of silicon powder, and the detailed description thereof is omitted here.
Based on the same technical concept, referring to fig. 2, fig. 2 is a schematic structural diagram of a tail gas treatment system in polysilicon production according to an embodiment of the present disclosure, as shown in fig. 2, the system includes:
the first separation device 1 is used for obtaining mixed gas to be treated and carrying out preliminary spraying and washing on the mixed gas to be treated to obtain first treated mixed gas and silicon powder solid slag;
the quenching tower 2 is connected with the first separation device 1 and is used for obtaining the first treated mixed gas and spraying and washing the first treated mixed gas to obtain a first chlorosilane gas and a chlorosilane residual liquid containing impurities;
the collecting device 3 is connected with the quenching tower and is used for collecting the first chlorosilane gas, condensing the first chlorosilane gas into first liquid-phase chlorosilane and then conveying the first liquid-phase chlorosilane to the first separating device 1, so that the first separating device 1 utilizes the first liquid-phase chlorosilane to spray and wash the mixed gas to be treated;
the second separation device 4 is respectively connected with the quenching tower 2 and the residue treatment device 7, and is used for performing solid-liquid separation on the chlorosilane residual liquid to obtain a chlorosilane clear liquid and a silicon powder turbid liquid, and also used for conveying the chlorosilane clear liquid to the quenching tower 2, so that the quenching tower 2 performs spray washing on the first treatment mixed gas by using the chlorosilane clear liquid; and the number of the first and second groups,
and the residue treatment device 7 is respectively connected with the first separation device 1 and the second separation device 4 and is used for collecting and treating the silicon powder solid residues from the first separation device 1 and the silicon powder turbid liquid from the second separation device 4.
In this embodiment, the second separating device 4 is a cyclone separator.
The cyclone separator can be used for separating liquid from solid, the working principle of the cyclone separator is that solid particles or liquid drops with larger inertial centrifugal force are thrown to the outer wall surface to be separated by the rotary motion caused by the tangential introduction of airflow, the embodiment utilizes the characteristics of the cyclone separator to realize the solid-liquid separation of chlorosilane clear liquid and silicon powder turbid liquid in chlorosilane residual liquid in the production process of polycrystalline silicon, utilizes the cyclone separator to treat the chlorosilane residual liquid, can completely separate impurities such as silicon powder, metal chloride and the like in the residual liquid from the chlorosilane clear liquid to obtain the upper chlorosilane clear liquid and the lower silicon powder turbid liquid, wherein the chlorosilane turbid solution contains a trace amount of chlorosilane clear solution and a large amount of silicon powder and metal chloride solid impurities, the chlorosilane clear liquid is recycled, the solid content is greatly reduced at the moment, and the turbid liquid of the silicon powder is subjected to next treatment. In addition, the cyclone separator has the characteristics of simple structure, large operation elasticity, high efficiency, convenient management and maintenance, low cost and the like, and can solve the problem of consideration of the cost of the polysilicon production process by various manufacturers.
Therefore, in the embodiment, by using the cyclone separation principle of the cyclone separator, solid-liquid separation is performed on the chlorosilane silicon powder mixed residual liquid at the kettle of the quenching tower, the upper chlorosilane clear liquid is circulated by the circulating pump of the quenching tower, and the lower silicon powder turbid liquid is further treated and discharged to realize solid-liquid separation, so that the solid content of the upper chlorosilane clear liquid is almost zero, and the circulating pump of the quenching tower cannot cause the problems of impeller abrasion, volute abrasion and the like due to conveying of solid slag, thereby achieving the purpose of prolonging the service cycle of the circulating pump of the quenching tower; on the other hand, the turbid liquid of the silicon powder after cyclone separation has higher solid content, and the concentration efficiency of the slag slurry can be improved.
In this embodiment, the first separation device 1 includes a venturi quench tank 1a and a venturi separation tank 1 b.
The venturi quenching tank 1a is respectively connected with the venturi separation tank 1b and the residue treatment device 7, and is used for obtaining a mixed gas to be treated and carrying out primary spraying and washing on the treated mixed gas to obtain a second treated mixed gas and silicon powder solid residues; and the number of the first and second groups,
the venturi quenching tank 1a is also used for conveying the second processing mixed gas to the venturi separation tank 1b and discharging the silicon powder solid slag to the slag processing device;
the venturi separation tank 1b is respectively connected with the venturi quenching tank 1a and the quenching tower 2, and is used for obtaining the second treated mixed gas and performing secondary spraying and washing on the second treated mixed gas to obtain the first treated mixed gas and the silicon powder solid slag; and the number of the first and second groups,
the venturi separation tank 1b is further configured to convey the first processed mixed gas to the quenching tower 2, and discharge the solid silicon powder slag to the slag treatment device 7.
Wherein, the spray washing of the venturi quenching tank 1a and the venturi separation tank 1b is realized by the washing and separation through chlorosilane spraying.
In one embodiment, the system further comprises: and the quenching tower circulating pump 5 is respectively connected with the quenching tower 2 and the second separation device 4, and is used for pressurizing and conveying the chlorosilane clear liquid output by the second separation device 4 to the quenching tower 2, so that the first treatment mixed gas is sprayed and washed by the pressurized chlorosilane clear liquid in the quenching tower 2.
In this embodiment, the circulating pump 5 of the quenching tower can adopt an open impeller; the motor of the circulating pump 5 of the quenching tower can adopt a frequency conversion mode; the circulating pump 5 of the quenching tower can be made of alloy materials.
In this embodiment, not only through handling the gas mixture and to chlorosilane raffinate in order to reduce its solid content, combine the corresponding improvement to the quench tower circulating pump simultaneously, make the quench tower circulating pump reach maximum operation cycle, change the impeller into open, in order to alleviate the wearing and tearing of impeller, change traditional stainless steel material into the wear-resisting material of alloy, can also change the frequency conversion mode into with quench tower circulating pump motor fixed frequency operation, and is further, can control the steady flow of quench tower circulating pump through the converter.
In one embodiment, the collecting device 3 comprises:
a first cooler 31 for cooling the first chlorosilane gas to obtain first liquid-phase chlorosilane;
a condensate intermediate tank 32 for collecting the first liquid phase chlorosilane and conveying the first liquid phase chlorosilane to the first separation device 1.
In one embodiment, the collecting device 3 further comprises: and a condensate intermediate tank reflux pump 33 which is respectively connected with the condensate intermediate tank 32 and the first separation device 1 and is used for pressurizing the first liquid-phase chlorosilane output by the condensate intermediate tank 32 and then conveying the pressurized first liquid-phase chlorosilane to the first separation device 1.
In one embodiment, the system further comprises:
the transfer tank 6 is connected between the first separation device 1 and the residue treatment device 7, and is used for flashing the silicon powder solid residue to generate second chlorosilane gas;
the filter 8 is connected with the transfer tank 6 and used for introducing the second chlorosilane gas and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen to obtain filtered second chlorosilane gas and hydrogen mixed gas;
the second cooler 9 is connected with the filter 8, and is used for cooling the second chlorosilane gas and hydrogen gas mixed gas to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
the liquid seal device 10 is respectively connected with the second cooler 9 and the transfer tank 6, and is used for recovering the second liquid-phase chlorosilane and returning the second liquid-phase chlorosilane to the transfer tank 6; and the number of the first and second groups,
a hydrogen make-up pre-tank 11, the hydrogen make-up pre-tank 11 being connected to the second cooler 9 for recovering the gaseous hydrogen.
In another embodiment, the system further comprises:
the transfer tank 6 is connected between the second separation device 4 and the residue treatment device 7, and is used for flashing the silicon powder turbid liquid to generate a second chlorosilane gas;
the filter 8 is connected with the transfer tank 6 and used for introducing the second chlorosilane gas and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen to obtain filtered second chlorosilane gas and hydrogen mixed gas;
the second cooler 9 is connected with the filter 8, and is used for cooling the second chlorosilane gas and hydrogen gas mixed gas to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
the liquid seal device 10 is respectively connected with the second cooler 9 and the transfer tank 6, and is used for recovering the second liquid-phase chlorosilane and returning the second liquid-phase chlorosilane to the transfer tank 6; and the number of the first and second groups,
a hydrogen make-up pre-tank 11, the hydrogen make-up pre-tank 11 being connected to the second cooler 9 for recovering the gaseous hydrogen.
Further, the system further comprises: and the silicon powder storage tank 12 is connected between the second separation device 4 and the transfer tank 6 and is used for depositing the turbid liquid of silicon powder and introducing the deposited turbid liquid of silicon powder into the transfer tank 6.
It should be noted that, the structures of the exhaust gas treatment system provided in the embodiment of the present disclosure have been described in detail in the above method embodiments, and are not described herein again.
In summary, in the method and system for treating tail gas in polysilicon production provided by the embodiment of the present disclosure, a mixed gas to be treated is introduced into a first separation device, the mixed gas to be treated is primarily sprayed and washed in the first separation device, the mixed gas subjected to the primary spraying and washing is introduced into a quenching tower, solid impurities containing a large amount of silicon powder and other metal chlorides are washed, solid content in the mixed gas is reduced, after the mixed gas enters the quenching tower for quenching, chlorosilane residual liquid at the bottom of the quenching tower is subjected to solid-liquid separation by using a second separation device, the residual solid impurities are separated from chlorosilane liquid, at this time, the separated chlorosilane clear liquid is conveyed to an inlet of a circulating pump of the quenching tower and is circulated to the quenching tower by the circulating pump, and in this process, solid impurities such as the silicon powder residual liquid and the metal chlorides are deposited in the silicon powder solid slag and the silicon powder turbid liquid, the solid content of the chlorosilane is greatly reduced, the problems that the operation of a quenching tower is abnormal due to overhigh solid content of the chlorosilane, the operation period of a circulating pump of the quenching tower is shortened and the like in the related technology are solved, and meanwhile, the overhaul cost is reduced; furthermore, a first cooler and a condensate intermediate tank are arranged between the quenching tower and the first separation device, the first cooler is used for condensing gas-phase chlorosilane to obtain first liquid-phase chlorosilane, the first liquid-phase chlorosilane is circulated by a condensate intermediate tank reflux pump, and mixed gas in the first separation device is sprayed and washed, so that the tail gas treatment efficiency in the production of polycrystalline silicon is improved, and the resource utilization rate is improved; furthermore, the solid slag and the turbid liquid of the silicon powder are treated by arranging a transfer tank, and chlorosilane is further recovered, so that the production cost is further reduced.
Finally, it should be noted that: the above embodiments are only used for illustrating the technical solutions of the present disclosure, and not for limiting the same; while the present disclosure has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present disclosure.
Claims (13)
1. A tail gas treatment method in polycrystalline silicon production is characterized by comprising the following steps:
introducing the mixed gas to be treated into a first separation device, and carrying out primary spraying and washing on the mixed gas to be treated in the first separation device to obtain first treated mixed gas and silicon powder solid slag;
discharging the silicon powder solid slag to a residue treatment device; and the number of the first and second groups,
introducing the first treated mixed gas into a quenching tower, and spraying and washing the first treated mixed gas in the quenching tower to obtain a first chlorosilane gas and a chlorosilane residual liquid containing impurities;
collecting the first chlorosilane gas, condensing the first chlorosilane gas into first liquid-phase chlorosilane, and conveying the first liquid-phase chlorosilane to the first separation device; and the number of the first and second groups,
introducing the chlorosilane residual liquid into a second separation device, and carrying out solid-liquid separation on the chlorosilane residual liquid in the second separation device to obtain a chlorosilane clear liquid and a silicon powder turbid liquid;
conveying the chlorosilane clear liquid to a quenching tower; and the number of the first and second groups,
and discharging the silicon powder turbid liquid to a residue treatment device.
2. The method according to claim 1, wherein the mixed gas to be treated is subjected to preliminary spray washing in the first separation device to obtain a first treated mixed gas and silicon powder solid slag, and the steps are as follows:
carrying out primary spraying and washing on the treated mixed gas in the first separation device to obtain a second treated mixed gas and silicon powder solid slag; and the number of the first and second groups,
and carrying out secondary spraying and washing on the second treated mixed gas in the first separation device to obtain the first treated mixed gas and silicon powder solid slag.
3. The method according to claim 1, further comprising, before discharging the silicon powder solid slag to a residue processing device:
discharging the silicon powder solid slag to a transfer tank, and flashing the silicon powder solid slag in the transfer tank to obtain second chlorosilane gas; and the number of the first and second groups,
introducing the second chlorosilane gas into a filter, and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen in the filter to obtain filtered second chlorosilane gas and hydrogen mixed gas;
introducing the filtered second chlorosilane gas and hydrogen mixed gas into a second cooler, and cooling the second chlorosilane gas and hydrogen mixed gas in the second cooler to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
introducing the second liquid-phase chlorosilane into a liquid seal device for recycling; and the number of the first and second groups,
and introducing the gas-phase hydrogen into a hydrogen make-up foretank for recycling.
4. The method according to claim 1, further comprising, before discharging the turbid liquid of silicon powder to a residue treatment device:
discharging the silicon powder turbid liquid to a transfer tank, and flashing the silicon powder turbid liquid in the transfer tank to obtain second chlorosilane gas; and the number of the first and second groups,
introducing the second chlorosilane gas into a filter, and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen in the filter to obtain filtered second chlorosilane gas and hydrogen mixed gas;
introducing the filtered second chlorosilane gas and hydrogen mixed gas into a second cooler, and cooling the second chlorosilane gas and hydrogen mixed gas in the second cooler to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
introducing the second liquid-phase chlorosilane into a liquid seal device for recycling; and the number of the first and second groups,
and introducing the gas-phase hydrogen into a hydrogen make-up foretank for recycling.
5. A tail gas treatment system in polycrystalline silicon production is characterized by comprising:
the first separation device is used for obtaining mixed gas to be treated and carrying out primary spraying and washing on the mixed gas to be treated to obtain first treated mixed gas and silicon powder solid slag;
the quenching tower is connected with the first separation device and used for obtaining the first treated mixed gas and spraying and washing the first treated mixed gas to obtain a first chlorosilane gas and a chlorosilane residual liquid containing impurities;
the collecting device is connected with the quenching tower and is used for collecting the first chlorosilane gas, condensing the first chlorosilane gas into first liquid-phase chlorosilane and conveying the first liquid-phase chlorosilane to the first separating device;
the second separation device is respectively connected with the quenching tower and the residue treatment device, is used for carrying out solid-liquid separation on the chlorosilane residual liquid to obtain a chlorosilane clear liquid and a silicon powder turbid liquid, and is also used for conveying the chlorosilane clear liquid to the quenching tower; and the number of the first and second groups,
and the residue treatment device is respectively connected with the first separation device and the second separation device and is used for collecting and treating the silicon powder solid residues from the first separation device and the silicon powder turbid liquid from the second separation device.
6. The system of claim 5, wherein the second separation device is a cyclone separator.
7. The system of claim 5, wherein the first separation device comprises a venturi quench tank and a venturi separation tank;
the Venturi quenching tank is respectively connected with the Venturi separation tank and the residue treatment device and is used for obtaining mixed gas to be treated and carrying out primary spraying and washing on the treated mixed gas to obtain second treated mixed gas and silicon powder solid residues; and the number of the first and second groups,
the Venturi quenching tank is also used for conveying the second processing mixed gas to the Venturi separation tank and discharging the silicon powder solid slag to the slag processing device;
the venturi separation tank is respectively connected with the venturi quenching tank and the quenching tower and is used for obtaining the second processing mixed gas and carrying out secondary spraying and washing on the second processing mixed gas to obtain the first processing mixed gas and silicon powder solid slag; and the number of the first and second groups,
the Venturi separation tank is also used for conveying the first treated mixed gas to the quenching tower and discharging the silicon powder solid slag to the slag treatment device.
8. The system of claim 5, further comprising: and the quenching tower circulating pump is respectively connected with the quenching tower and the second separation device and is used for pressurizing and conveying the chlorosilane clear liquid output by the second separation device to the quenching tower.
9. The system of claim 8, wherein the quench tower circulation pump employs an open impeller; and/or the circulating pump motor of the quenching tower adopts a frequency conversion mode; and/or the circulating pump of the quenching tower is made of alloy materials.
10. The system of claim 5, wherein the collection device comprises:
a first cooler for cooling the first chlorosilane gas to obtain a first liquid phase chlorosilane; and the number of the first and second groups,
and the condensate intermediate tank is used for collecting the first liquid-phase chlorosilane and conveying the first liquid-phase chlorosilane to the first separation device.
11. The system of claim 5, further comprising:
the transfer tank is connected between the first separation device and the residue treatment device and is used for flashing the silicon powder solid residue into second chlorosilane gas;
the filter is connected with the transfer tank and is used for introducing the second chlorosilane gas and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen to obtain filtered second chlorosilane gas and hydrogen mixed gas;
the second cooler is connected with the filter and used for cooling the second chlorosilane gas and hydrogen mixed gas to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
the liquid seal device is respectively connected with the second cooler and the transfer tank and is used for recovering the second liquid-phase chlorosilane and returning the second liquid-phase chlorosilane to the transfer tank; and the number of the first and second groups,
a make-up hydrogen front tank connected to the second cooler for recovering the gas-phase hydrogen gas.
12. The system of claim 5, further comprising:
the transfer tank is connected between the second separation device and the residue treatment device and is used for flashing the turbid liquid of the silicon powder out of a second chlorosilane gas;
the filter is connected with the transfer tank and is used for introducing the second chlorosilane gas and filtering impurities in the second chlorosilane gas by using high-pressure hydrogen to obtain filtered second chlorosilane gas and hydrogen mixed gas;
the second cooler is connected with the filter and used for cooling the second chlorosilane gas and hydrogen mixed gas to obtain second liquid-phase chlorosilane and gas-phase hydrogen;
the liquid seal device is respectively connected with the second cooler and the transfer tank and is used for recovering the second liquid-phase chlorosilane and returning the second liquid-phase chlorosilane to the transfer tank; and the number of the first and second groups,
a make-up hydrogen front tank connected to the second cooler for recovering the gas-phase hydrogen gas.
13. The system of claim 12, further comprising: and the silicon powder storage tank is respectively connected with the second separation device and the transfer tank and is used for depositing the silicon powder turbid liquid and introducing the deposited silicon powder turbid liquid into the transfer tank.
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